CN106732214A - A kind of hydrophobicity natural polymer/attapulgite composite aerogel and preparation method thereof - Google Patents
A kind of hydrophobicity natural polymer/attapulgite composite aerogel and preparation method thereof Download PDFInfo
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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Abstract
The invention discloses a kind of hydrophobicity natural polymer/attapulgite composite aerogel preparation method, natural polymer is first specially dissolved in water and obtains clear solution, attapulgite and organosilicon modifier are then added in the solution, freezed after stirring.Vacuum freeze drying is carried out again obtains corresponding hydrophobicity natural polymer/attapulgite composite aerogel.Its pore-size distribution is 2 ~ 700 nm, and BET specific surface area is up to 30 ~ 800 m2·g‑1, apparent density is 0.02 ~ 0.35 gcm‑3, thermal conductivity is 0.01 ~ 0.05 Wm‑1·k‑1, modulus of compressibility is 0.05 ~ 10 MPa, and contact angle is 90 ° ~ 179.9 °, and combustion heat value is 0.6 ~ 1.9 MJ kg‑1.Natural polymer/attapulgite composite aerogel prepared by the present invention is blockiness good, and hydrophobicity is good, and density is low, and intensity is high, and thermal conductivity is low, and combustion heat value is less than 1.9MJ kg‑1, reached A grades of fire-retardant requirement；Preparation process is simple, cycle is short is pollution-free.Hydrophobicity natural polymer/attapulgite the composite aerogel of preparation can be applied to the fields such as building energy conservation, petrochemical industry, sewage disposal.
Description
Technical field
It is multiple the invention belongs to new chemical materialses preparation field, more particularly to a kind of hydrophobicity natural polymer/attapulgite
Close aeroge and preparation method thereof.
Background technology
Aeroge is a kind of functional material of three-dimensional porous structure, generally by sol-gel and supercritical drying process
Prepare, be the heat preserving and insulating material of a class superior performance, in fields such as building, industry the features such as with lightweight, extremely low thermal conductivity
With important research and application value.Current most study is silica and its composite aerogel, and the aerogel-like leads to
Often with organosilicon as presoma, prepared using Supercritical Drying Technology after sol-gel.Due to organosilan price, surpass
Critical drying needs the expensive devices such as autoclave, and preparation technology is complicated, the cycle is long, causes aeroge preparation cost high.Industrially
Using the aerosil heat insulation felt price of the technique productions at 30,000 yuan every cube or so, be in the market conventional vacuum every
More than ten times of hot material price.Expensive price makes it very difficult in the civil area application such as building heat preservation.To solve to make
Standby problem with high costs, in recent years, researchers both domestic and external develop constant pressure and dry technique, after gel is prepared, warp
Directly dried in atmospheric conditions after multiple exchange of solvent, surface hydrophobicity modification procedure.The technique is low for equipment requirements, but
Because constant pressure and dry process can not be eliminated because of the capillary force action that gas-liquid interface is produced, cause the aeroge shrinkage cracking for preparing
Seriously, it is difficult to prepare complete large scale aeroge, and the technique needs more solvent to exchange and surface modification step, prepare
Cycle is long, is not made a breakthrough also in industrialized production.On the other hand, aerosil itself poor mechanical property, fragility
Greatly, its structure is susceptible to cave under the effect of less external force, and aerogel heat-proof felt in the market is in work progress
It is also easy to produce dust, is detrimental to health.
Accordingly, it would be desirable to developing new aeroge has solved the problems, such as above-mentioned aerosil, United States Patent (USP)
US3203903 is reported and is added clay in the polymer, and it is good to prepare dimensionally stable, mechanical property by the method for freeze-drying
Aerogel composite, the aeroge of preparation is hydrophily aeroge.United States Patent (USP) US20070208124 is reported will be polymerized
Thing, clay, binding agent are prepared for the aerogel composite with nano-pore after being mixed by the method for freeze-drying, but
Because polymer and binder content are high, the fire resistance of composite aerogel is poor, does not reach building thermal insulation material to anti-flammability
The requirement of energy.Chen et al. is reported and is added nano inorganic mineral montmorillonite, bentonite, kaolin in poly-vinyl alcohol solution
Improve the anti-flammability of composite aerogel（Chen H B, Wang Y Z, Schiraldi D A. Preparation and
Flammability of Poly(vinyl alcohol) Composite Aerogels[J]. Acs Applied
Materials & Interfaces, 2014, 6(9):6790-6796.）, but mechanical property do not report for work.Wang et al. will gather
Vinyl alcohol adds ammonium polyphosphate fire retardant while improve the mechanical property and anti-flammability of aeroge after mixing with sodium montmorillonite
Energy（Wang Y T, Liao S F, Shang K, et al. Efficient Approach to Improving the
Flame Retardancy of Poly(vinylalcohol)/Clay Aerogels: Incorporating
Piperazine-Modified Ammonium Polyphosphate[J]. Acs Applied Materials &
Interfaces, 2015, 7(3):1780-1786.）.Chinese patent CN103113043 is reported in inorganic micro-and nano-particles
The mechanical property of composite aerogel is improved with crosslinkable polymer and reinforcing fiber is added in the mixed solution of polymer,
But need by follow-up solidification cross-linking step.In addition, the composite aerogel of above-mentioned report is due to using soluble polymer
Make aeroge that there is hydrophily, aeroge can be caused to absorb moisture in use and make the performance such as thermal insulation of aeroge
Energy, mechanical property etc. decline.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, there is provided a kind of hydrophobicity natural polymer/concave convex rod
Stone composite aerogel, it is compound it is a further object of the present invention to provide a kind of hydrophobicity natural polymer/attapulgite of the invention
The preparation method of aeroge.
The technical scheme is that：
A kind of preparation method of hydrophobicity natural polymer/attapulgite composite aerogel, comprises the following steps：
Step one, natural polymer is dissolved in water obtains solution, attapulgite is added in the solution and organosiloxane is hydrophobic changes
Property agent, after stirring freeze obtaining solid；
Step 2, the solid for obtaining above-mentioned freezing are carried out being vacuum dried below -10 DEG C and obtain hydrophobicity natural polymer/recessed
Convex rod stone composite aerogel；
The mass ratio of the natural polymer, attapulgite, organosiloxane hydrophobic modifier and water is 1: 1~40 : 1~5 :
20 ~ 100, preferably 1: 10~30 : 2~4 : 40~80.
Cryogenic temperature described in step one is -40 ~ -196 DEG C.
Step 2 is that the h of vacuum drying 24 ~ 96 is carried out at -10 DEG C to -90 DEG C.
Further improvement of the present invention scheme is：
The natural polymer be wheaten starch, potato starch, sweet potato starch, cornstarch, sodium alginate, shitosan, agar-agar,
In Arabic gum, rubber made from soybean cake, locust bean gum, tragacanth gum, gelatine, gelatin, casein, guanidine glue, xanthans or water soluble protein
One or more mixing.
The organosiloxane hydrophobic modifier is MTMS, dimethyldimethoxysil,ne, methyl three
Ethoxysilane, dimethyldiethoxysilane, ethyl trimethoxy silane, diethyldimethoxysilane, diethyl diethyl
TMOS, vinyltrimethoxy silane, VTES, methylvinyldimethoxysilane, hexamethyl
Disiloxane, seven tetramethyldisiloxanes, octyltri-ethoxysilane, chloropropyl triethoxysilane, methyl trichlorosilane, diformazan
One or more mixing in base dichlorosilane, ethyl trichlorosilane or diethyl dichlorosilane.
Preferably MTMS, MTES, ethyl trimethoxy silane, ethyl triethoxy
One or more mixing in silane, vinyltrimethoxy silane or VTES.
Further improvement project of the invention is：
A kind of hydrophobicity natural polymer/attapulgite composite aerogel is in building, petrochemical industry or dirt obtained in the above method
The application of water treatment field.
Beneficial effects of the present invention are：
1. the aerogel material that the present invention is provided employs natural polymer as matrix material, with cheap, originates wide
It is general, the green non-poisonous advantage of raw material；
2. the aerogel material that the present invention is provided employs attapulgite as inorganic compounding phase, because attapulgite is in water
With good colloidal stability, therefore any dispersant need not be added in preparation process；Attapulgite has and receives simultaneously
The characteristic of rice fibre structure and inorganic mineral, can play enhancing and fire-retardant effect in composite aerogel.
3. the aeroge that the present invention is provided with the addition of the organosiloxane containing hydrophobic grouping, organosiloxane by hydrolysis,
Polycondensation reaction is modified to aeroge surface, introduces hydrophobic grouping, and the presence of hydrophobic grouping imparts aeroge hydrophobicity, makes
Moisture is not absorbed during, structure and the stable performance of aeroge can be kept.
4. any organic solvent is not used in the preparation method that the present invention is provided, and without waste water,waste gas and industrial residue discharge, is met
Environment protection requirement；And preparation method is simple, it is with low cost, be easy to industrialized production.
5. composite aerogel of the invention, its pore-size distribution is 2 ~ 700 nm, and BET specific surface area is up to 30 ~ 800 m2·
g-1, density is 0.02 ~ 0.35 gcm-3, thermal conductivity is 0.01 ~ 0.05 Wm-1·k-1, modulus of compressibility is 0.05 ~ 10 MPa,
Contact angle is 90 ° ~ 179.9 °, and combustion heat value is 0.6 ~ 1.9 MJ kg-1.The apparent density is preferably 0.05 ~ 0.20 g
cm-3。
Brief description of the drawings
Fig. 1 is the outside drawing of hydrophobicity natural polymer/attapulgite composite aerogel prepared by embodiment 2, from figure
As can be seen that complete block aeroge can be prepared by the method.
Fig. 2 is the contact angle figure of hydrophobicity natural polymer/attapulgite composite aerogel prepared by embodiment 2, from figure
In as can be seen that by adding the organosiloxane containing hydrophobic grouping hydrophobic aeroge can be obtained, and contact angle is 120 °.
Fig. 3 is the micro-structure diagram of hydrophobicity natural polymer/attapulgite composite aerogel prepared by embodiment 2, from
It can be seen that composite aerogel has nano-porous structure in figure.
Specific embodiment
Embodiment 1
Shitosan is dissolved in water and obtains clear solution, attapulgite and MTMS are added in the solution, stirring is equal
At -196 DEG C freeze after even obtaining solid；The solid that obtains will be freezed 24 h of vacuum drying will be carried out at -90 DEG C and obtained
To hydrophobicity natural polymer/attapulgite composite aerogel；Wherein shitosan, attapulgite, MTMS with
The mass ratio of water is 1:5:2:80；
The density of the hydrophobicity natural polymer/attapulgite composite aerogel of preparation is 0.05 gcm-3, use nitrogen adsorption
Method gaging hole footpath is distributed as 50 ~ 700 nm, and BET specific surface area is up to 30 m2·g-1, it is 0.02 that plane heat source method measures thermal conductivity
W·m-1·k-1, modulus of compressibility is measured for 0.05 MPa with universal testing machine, contact angle is measured for 115 ° with contact angle measurement,
It is 0.6MJ kg to measure combustion heat value with calorimeter-1。
Embodiment 2
Shitosan is dissolved in water and obtains clear solution, attapulgite and MTMS are added in the solution, stirring is equal
At -196 DEG C freeze after even obtaining solid；The solid that obtains will be freezed 48 h of vacuum drying will be carried out at -90 DEG C and obtained
To hydrophobicity natural polymer/attapulgite composite aerogel；Wherein shitosan, attapulgite, MTMS with
The mass ratio of water is 1:10:3:70；
The density of the hydrophobicity natural polymer/attapulgite composite aerogel of preparation is 0.10 gcm-3, use nitrogen adsorption
Method gaging hole footpath is distributed as 2 ~ 500 nm, and BET specific surface area is up to 300 m2·g-1, measuring thermal conductivity with Adsorbent By Using Transient Plane Source Technique is
0.01 W·m-1·k-1, modulus of compressibility is measured for 0.5 MPa with universal testing machine, measuring contact angle with contact angle measurement is
120 °, it is 0.9MJ kg to measure combustion heat value with calorimeter-1。
Embodiment 3
Cornstarch is dissolved in water and obtains clear solution, attapulgite and MTMS, stirring are added in the solution
At -60 DEG C freeze obtaining solid after uniform；The solid that obtains will be freezed 48 h of vacuum drying will be carried out at -10 DEG C and obtained
To hydrophobicity natural polymer/attapulgite composite aerogel；Wherein cornstarch, attapulgite, MTMS
It is 1 with the mass ratio of water:15:4:80；
The density of the hydrophobicity natural polymer/attapulgite composite aerogel of preparation is 0.15 gcm-3, use nitrogen adsorption
Method measures pore-size distribution for 10 ~ 400 nm, and BET specific surface area is up to 400 m2·g-1, thermal conductivity is measured with Adsorbent By Using Transient Plane Source Technique
Rate is 0.02 Wm-1·k-1, modulus of compressibility is measured for 2.5 MPa with universal testing machine, measure contact with contact angle measurement
Angle is 179.9 °, and combustion heat value is measured for 1.2 MJ kg with calorimeter-1。
Embodiment 4
Cornstarch is dissolved in water and obtains clear solution, attapulgite and MTES, stirring are added in the solution
At -40 DEG C freeze obtaining solid after uniform；The solid that obtains will be freezed 48 h of vacuum drying will be carried out at -10 DEG C and obtained
To hydrophobicity natural polymer/attapulgite composite aerogel；Wherein cornstarch, attapulgite, MTMS
It is 1 with the mass ratio of water:5:2:40；
The density of the hydrophobicity natural polymer/attapulgite composite aerogel of preparation is 0.20 gcm-3, use nitrogen adsorption
Method measures pore-size distribution for 10 ~ 200 nm, and BET specific surface area is up to 700 m2·g-1, thermal conductivity is measured with Adsorbent By Using Transient Plane Source Technique
Rate is 0.025 Wm-1·k-1, modulus of compressibility is measured for 5.8 MPa with universal testing machine, measure contact with contact angle measurement
Angle is 150 °, and combustion heat value is measured for 0.7 MJ kg with calorimeter-1。
Embodiment 5
Arabic gum is dissolved in water and obtains clear solution, attapulgite and MTES, stirring are added in the solution
At -40 DEG C freeze obtaining solid after uniform；The solid that obtains will be freezed 48 h of vacuum drying will be carried out at -10 DEG C and obtained
To hydrophobicity natural polymer/attapulgite composite aerogel；Wherein cornstarch, attapulgite, MTMS
It is 1 with the mass ratio of water:20:4:80；
The density of the hydrophobicity natural polymer/attapulgite composite aerogel of preparation is 0.30 gcm-3, use nitrogen adsorption
Method measures pore-size distribution for 2 ~ 200 nm, and BET specific surface area is up to 500 m2·g-1, thermal conductivity is measured with Adsorbent By Using Transient Plane Source Technique
It is 0.035 Wm-1·k-1, modulus of compressibility is measured for 10 MPa with universal testing machine, measure contact angle with contact angle measurement
It is 160 °, combustion heat value is measured for 1.9 MJ kg with calorimeter-1。
Claims (8)
1. a kind of preparation method of hydrophobicity natural polymer/attapulgite composite aerogel, it is characterised in that including following step
Suddenly：
Step one, natural polymer is dissolved in water obtains solution, attapulgite is added in the solution and organosiloxane is hydrophobic changes
Property agent, after stirring freeze obtaining solid；
Step 2, the solid for obtaining above-mentioned freezing are carried out being vacuum dried below -10 DEG C and obtain hydrophobicity natural polymer/recessed
Convex rod stone composite aerogel；
The mass ratio of the natural polymer, attapulgite, organosiloxane hydrophobic modifier and water is 1: 1~40 : 1~5 :
20~100。
2. hydrophobicity natural macromolecular material/attapulgite composite aerogel according to claim 1, it is characterised in that
The mass ratio of the natural polymer, attapulgite, organosiloxane hydrophobic modifier and water is 1: 10~30 : 2~4 : 40
~80。
3. hydrophobicity natural macromolecular material/attapulgite composite aerogel according to claim 1, it is characterised in that
Cryogenic temperature described in step one is -40 ~ -196 DEG C.
4. hydrophobicity natural macromolecular material/attapulgite composite aerogel according to claim 1, it is characterised in that
Step 2 is that the h of vacuum drying 24 ~ 96 is carried out at -10 DEG C to -90 DEG C.
5. hydrophobicity natural macromolecular material/attapulgite composite aerogel according to claim 1 and 2, its feature exists
In, the natural polymer be wheaten starch, potato starch, sweet potato starch, cornstarch, sodium alginate, shitosan, agar-agar,
In Arabic gum, rubber made from soybean cake, locust bean gum, tragacanth gum, gelatine, gelatin, casein, guanidine glue, xanthans or water soluble protein
One or more mixing.
6. hydrophobicity natural macromolecular material/attapulgite composite aerogel according to claim 1 and 2, its feature exists
In the organosiloxane hydrophobic modifier is MTMS, dimethyldimethoxysil,ne, methyl triethoxy
Silane, dimethyldiethoxysilane, ethyl trimethoxy silane, diethyldimethoxysilane, diethyl diethoxy silicon
Alkane, vinyltrimethoxy silane, VTES, methylvinyldimethoxysilane, the silica of hexamethyl two
Alkane, seven tetramethyldisiloxanes, octyltri-ethoxysilane, chloropropyl triethoxysilane, methyl trichlorosilane, dimethyl dichloro
One or more mixing in silane, ethyl trichlorosilane or diethyl dichlorosilane.
7. hydrophobicity natural macromolecular material/attapulgite composite aerogel according to claim 1 and 2, its feature exists
In described organosiloxane hydrophobic modifier is MTMS, MTES, ethyl trimethoxy
In silane, ethyl triethoxysilane, vinyltrimethoxy silane or VTES one or two with
Upper mixing.
8. a kind of hydrophobicity natural polymer/attapulgite composite aerogel obtained in any one of claim 1 to 7 building,
The application of petrochemical industry or sewage treatment area.
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| CN107055508A (en) * | 2017-06-20 | 2017-08-18 | 盐城工学院 | Porous carbon aerogel material and preparation method thereof |
| CN107185515A (en) * | 2017-06-28 | 2017-09-22 | 郑善 | It is a kind of for photochemical catalyst of sewage disposal and preparation method thereof |
| CN108273476A (en) * | 2018-03-05 | 2018-07-13 | 西北师范大学 | A kind of preparation method of the compound porous hydrophobic oil suction sponge material of zein-sodium alginate |
| CN108975794A (en) * | 2018-09-11 | 2018-12-11 | 淮阴工学院 | Clay/sodium alginate composite aerogel fire proofing and preparation method thereof |
| CN109078588A (en) * | 2018-09-11 | 2018-12-25 | 淮阴工学院 | Recessed native composite aerogel of extremely-low density sodium alginate-and preparation method thereof |
| CN109126644A (en) * | 2017-06-15 | 2019-01-04 | 湖南尚成新材料科技有限责任公司 | A kind of high-damping aerogel composite and preparation method thereof |
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| CN107185515A (en) * | 2017-06-28 | 2017-09-22 | 郑善 | It is a kind of for photochemical catalyst of sewage disposal and preparation method thereof |
| CN108273476A (en) * | 2018-03-05 | 2018-07-13 | 西北师范大学 | A kind of preparation method of the compound porous hydrophobic oil suction sponge material of zein-sodium alginate |
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